CN111785795B - ZnMgGaO ultraviolet detector and preparation method thereof - Google Patents
ZnMgGaO ultraviolet detector and preparation method thereof Download PDFInfo
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- CN111785795B CN111785795B CN202010800925.XA CN202010800925A CN111785795B CN 111785795 B CN111785795 B CN 111785795B CN 202010800925 A CN202010800925 A CN 202010800925A CN 111785795 B CN111785795 B CN 111785795B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000001301 oxygen Substances 0.000 claims abstract description 28
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 239000011701 zinc Substances 0.000 claims abstract description 23
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 19
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 19
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 19
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 19
- 239000011777 magnesium Substances 0.000 claims abstract description 19
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 19
- 238000004544 sputter deposition Methods 0.000 claims abstract description 13
- 230000004298 light response Effects 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 9
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 8
- 238000001459 lithography Methods 0.000 claims abstract description 8
- 238000010521 absorption reaction Methods 0.000 claims abstract description 7
- 150000002259 gallium compounds Chemical class 0.000 claims abstract description 7
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 7
- 150000002902 organometallic compounds Chemical class 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 150000003752 zinc compounds Chemical class 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 239000012159 carrier gas Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 7
- KZLUHGRPVSRSHI-UHFFFAOYSA-N dimethylmagnesium Chemical compound C[Mg]C KZLUHGRPVSRSHI-UHFFFAOYSA-N 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- AXAZMDOAUQTMOW-UHFFFAOYSA-N dimethylzinc Chemical compound C[Zn]C AXAZMDOAUQTMOW-UHFFFAOYSA-N 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052596 spinel Inorganic materials 0.000 claims description 4
- 239000011029 spinel Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 235000011147 magnesium chloride Nutrition 0.000 claims description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 3
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims 1
- 238000005191 phase separation Methods 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 5
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 76
- 230000031700 light absorption Effects 0.000 description 10
- 238000007747 plating Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 229910052594 sapphire Inorganic materials 0.000 description 4
- 239000010980 sapphire Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 4
- 238000002083 X-ray spectrum Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 3
- DLPASUVGCQPFFO-UHFFFAOYSA-N magnesium;ethane Chemical compound [Mg+2].[CH2-]C.[CH2-]C DLPASUVGCQPFFO-UHFFFAOYSA-N 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000002901 organomagnesium compounds Chemical class 0.000 description 2
- 238000000825 ultraviolet detection Methods 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 229910003363 ZnMgO Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0328—Inorganic materials including, apart from doping materials or other impurities, semiconductor materials provided for in two or more of groups H01L31/0272 - H01L31/032
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02554—Oxides
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors characterised by potential barriers, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
- H01L31/102—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier
- H01L31/108—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier the potential barrier being of the Schottky type
- H01L31/1085—Devices sensitive to infrared, visible or ultraviolet radiation characterised by only one potential barrier the potential barrier being of the Schottky type the devices being of the Metal-Semiconductor-Metal [MSM] Schottky barrier type
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Abstract
The invention provides a ZnMgGaO ultraviolet detector and a preparation method thereof, wherein the method comprises the following steps: s1, growing ZnMgGaO films on the surface of a substrate by using a metal organic compound chemical vapor deposition method by taking an organic zinc compound as a zinc source, an organic magnesium compound as a magnesium source, an organic gallium compound as a gallium source and high-purity oxygen as an oxygen source; s2, forming an interdigital electrode mask on the ZnMgGaO film by using negative photoresist lithography, and removing the interdigital electrode mask after sputtering metal to form an interdigital electrode; and S3, pressing In particles on the interdigital electrodes to obtain the ZnMgGaO ultraviolet detector with the MSM structure. Compared with the prior art, the preparation method provided by the invention has the advantages that the ZnMgGaO film is prepared by using the metal organic compound chemical vapor deposition method, and the prepared ZnMgGaO film has the characteristics of high crystallization quality, no phase separation, steep absorption cut-off edge and the like by increasing the oxygen flow, increasing the oxygen partial pressure and reducing the oxygen defects, so that the ultraviolet detector containing the ZnMgGaO film has lower dark current and faster light response speed.
Description
Technical Field
The invention relates to the technical field of semiconductor ultraviolet detection, in particular to a ZnMgGaO ultraviolet detector and a preparation method thereof.
Background
The ultraviolet detection technology has wide application prospect in military and civil fields such as missile tail flame detection, flame sensing, air and water purification, air-to-air communication and the like. Ultraviolet radiation having a wavelength less than 280nm is almost impossible to transmit to the earth's surface due to the blocking of the earth's above-earth ozone layer, and is called solar blind ultraviolet. The solar blind ultraviolet detector working in the solar blind wave band is not interfered by solar radiation, has higher sensitivity, and can be applied to missile early warning and the like. In recent years, the wide bandgap semiconductor ultraviolet detector is considered to be a third generation ultraviolet detector capable of replacing a vacuum photomultiplier and a Si photomultiplier because of the advantages of small size, light weight, no need of an optical filter during operation, no need of refrigeration and the like.
ZnMgGaO is a composite oxide of ZnO, mgO and Ga 2O3, has a spinel structure, belongs to a direct band gap semiconductor, has a forbidden band width of 3.4-7.8 eV, and can be applied to ultraviolet light electric devices in 160-368 nm in principle. Compared with ZnMgO, znMgGaO has similar ionic radiuses of Zn 2+、Mg2+ and Ga 2+, more adjustable selectivity of the band gap of the material can be realized by adjusting the components of the Zn 2+、Mg2+ and Ga 2+, and meanwhile, the problem of structural phase separation can be avoided; znMgGaO compared with Ga 2O3, can realize electrical property regulation and control, promote conductivity. And also has the advantages of good stability, good radiation resistance, low dark current and the like due to ZnMgGaO. Therefore ZnMgGaO is a candidate material for preparing a solar blind ultraviolet detector.
ZnMgGaO films are typically prepared by pulsed laser deposition and radio frequency magnetron sputtering. The ZnMgGaO thin film crystals prepared by the two methods have low quality and more defect states, so that the prepared ultraviolet detector has larger dark current and lower light response speed.
Disclosure of Invention
In order to solve the problems of low quality of ZnMgGaO thin film crystals prepared by pulse laser deposition and radio frequency magnetron sputtering, large dark current and low light response of an ultraviolet detector caused by more defect states, the invention provides a ZnMgGaO ultraviolet detector and a preparation method thereof, wherein a metal organic compound chemical vapor deposition method is used for preparing a ZnMgGaO thin film, so that the ZnMgGaO thin film has the advantages of high crystallization quality, no phase separation and steep absorption cut-off edge, and the ultraviolet detector comprising the ZnMgGaO thin film has low dark current and high light response speed.
In order to achieve the above purpose, the present invention adopts the following specific technical scheme:
the invention provides a ZnMgGaO ultraviolet detector which comprises a substrate, znMgGaO films and interdigital electrodes which are sequentially overlapped from bottom to top.
Preferably, znMgGaO films are spinel structures.
Preferably, the absorption cut-off edge of ZnMgGaO film is 220-280 nm, and the light response cut-off edge of ZnMgGaO ultraviolet detector is 220-270 nm.
The invention also provides a preparation method of the ZnMgGaO ultraviolet detector, which comprises the following steps:
S1, growing ZnMgGaO films on the surface of a substrate by using a metal organic compound chemical vapor deposition method by taking an organic zinc compound as a zinc source, an organic magnesium compound as a magnesium source, an organic gallium compound as a gallium source and high-purity oxygen as an oxygen source;
S2, forming an interdigital electrode mask on the ZnMgGaO film by using negative photoresist lithography, and removing the interdigital electrode mask after sputtering metal on the interdigital electrode mask to form an interdigital electrode;
and S3, pressing In particles on the interdigital electrodes to obtain the ZnMgGaO ultraviolet detector with the MSM structure.
Preferably, the flow rate of the high purity oxygen is 500 to 800sccm.
Preferably, the organozinc compound is dimethyl zinc or diethyl zinc; the organic magnesium compound is dimethyl magnesium and/or diethyl magnesium; the organic gallium compound is trimethyl gallium and/or triethyl gallium.
Preferably, the organozinc compound uses high-purity nitrogen as carrier gas, and the flow rate of the carrier gas is 5-20 sccm; the organomagnesium compound takes high-purity nitrogen as carrier gas, and the flow rate of the carrier gas is 5-20 sccm; the organogallium compound uses high-purity nitrogen as carrier gas, and the carrier gas flow rate is 10-40 sccm.
Preferably, in step S2, the sputtering current is 5 to 8mA.
Preferably, in step S2, the interdigital electrode mask is removed by using ultrasonic waves, and the ultrasonic time is 3-5 min.
Preferably, a secondary annealing step is further included after step S1, specifically as follows:
A. And (3) primary annealing: transferring ZnMgGaO film into annealing furnace, using nitrogen atmosphere, nitrogen flow rate is 0.6-1.0 sccm, raising furnace temperature of annealing furnace to 700-800 deg.C at heating rate of 0.2-0.4 deg.C/s, after 3-5 min, transferring ZnMgGaO film out of annealing furnace;
B. and (3) secondary annealing: and (3) reducing the temperature of the annealing furnace to 500-600 ℃, moving the ZnMgGaO film into the annealing furnace, and moving the ZnMgGaO film out of the annealing furnace after 15-20 min.
The invention can obtain the following technical effects:
the ZnMgGaO film is prepared by using a metal organic compound chemical vapor deposition method, and the prepared ZnMgGaO film has the characteristics of high crystallization quality, no phase separation, steep absorption cut-off edge and the like by increasing the oxygen flow, increasing the oxygen partial pressure and reducing the oxygen defects, so that an ultraviolet detector containing the ZnMgGaO film has lower dark current and faster light response speed.
Drawings
FIG. 1 is a schematic diagram of a ZnMgGaO UV detector according to the present invention;
FIG. 2 is a schematic flow chart of a method for manufacturing ZnMgGaO ultraviolet detector provided by the invention;
FIG. 3 is a graph showing the ultraviolet-visible light absorption spectrum of ZnMgGaO film of example 1 of the present invention;
FIG. 4 is a chart of the X-ray spectrum analysis of ZnMgGaO thin film of example 1 of the present invention;
FIG. 5 is a graph showing the current-voltage characteristics of ZnMgGaO UV detector of example 1 of the present invention;
FIG. 6 is a graph showing the current versus time characteristics of ZnMgGaO UV detector of example 1 of the present invention;
FIG. 7 is a graph showing the ultraviolet-visible light absorption spectrum of ZnMgGaO film of example 2 of the present invention;
FIG. 8 is a chart of the X-ray spectrum analysis of ZnMgGaO film of example 2 of the present invention;
FIG. 9 is a graph showing the current-voltage characteristics of ZnMgGaO UV detector of example 2 of the present invention;
FIG. 10 is a graph showing the current versus time characteristics of ZnMgGaO UV detector of example 2 of the present invention;
FIG. 11 is a graph showing the ultraviolet-visible light absorption spectrum of ZnMgGaO film of example 3 of the present invention;
FIG. 12 is a chart of the X-ray spectrum analysis of ZnMgGaO film of example 3 of the present invention;
FIG. 13 is a graph showing the current-voltage characteristics of ZnMgGaO UV detector of example 3 of the present invention;
FIG. 14 is a graph showing the current versus time characteristics of ZnMgGaO UV detector of example 3 of the present invention.
Wherein reference numerals include: a substrate 1, znMgGaO a film 2, an interdigital electrode 3 and In particles 4.
Detailed Description
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the following description, like modules are denoted by like reference numerals. In the case of the same reference numerals, their names and functions are also the same. Therefore, a detailed description thereof will not be repeated.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not to be construed as limiting the invention.
The scheme provided by the invention will be described in detail below with reference to the accompanying drawings.
Fig. 1 shows a structure of ZnMgGaO ultraviolet detector provided by the present invention.
As shown in fig. 1, the ZnMgGaO ultraviolet detector provided by the present invention includes: the substrate 1, znMgGaO film 2 and interdigital electrode 3 are stacked In this order from bottom to top, and In particles 4 are pressed on the interdigital electrode 3.
The substrate 1 is not particularly limited as long as it is a substrate well known to those skilled in the art, and is preferably a sapphire substrate in the present invention.
ZnMgGaO film 2 is spinel structure, belongs to direct band gap semiconductor, and has forbidden band width of 3.4-7.8 eV, so that ZnMgGaO ultraviolet detector can realize detection in shorter wave band. In addition, the ionic radiuses of the Zn 2+、Mg2+ and the Ga 2+ are similar, more adjustable selectivity of the band gap of the material can be realized through adjusting the components of the Zn 2+、Mg2+ and the Ga 2+, and meanwhile, the problem of structural phase separation can be avoided.
The light absorption cut-off edge of ZnMgGaO film 2 is 220-280 nm, and the absorption cut-off edge is very steep.
ZnMgGaO the thickness of the film 2 is 100-600 nm.
The light response cut-off edge of ZnMgGaO ultraviolet detector is 220-270 nm.
The preparation method of ZnMgGaO film 2 comprises the following steps: and heating the substrate to a certain temperature in an excessive oxygen atmosphere by utilizing Metal Organic Chemical Vapor Deposition (MOCVD) equipment, taking an organic zinc compound as a zinc source, taking an organic magnesium compound as a magnesium source and taking an organic gallium compound as a gallium source, and growing ZnMgGaO films on the substrate.
The preparation method of the interdigital electrode 3 comprises the following steps: forming an interdigital electrode mask on the ZnMgGaO film 2 by using negative photoresist photoetching, sputtering metal on the interdigital electrode mask by using a small-sized film plating machine, and removing the interdigital electrode mask by using an ultrasonic mode and the like to form the interdigital electrode.
The above details the structure of ZnMgGaO uv detector provided by the present invention. Corresponding to ZnMgGaO ultraviolet detector, the invention also provides a preparation method of ZnMgGaO ultraviolet detector.
Fig. 2 shows a flow of a method for manufacturing ZnMgGaO uv detector as provided by the present invention.
As shown in fig. 2, the preparation method of ZnMgGaO ultraviolet detector provided by the invention comprises the following steps:
S1, growing ZnMgGaO films on the surface of a substrate by using an organic zinc compound as a zinc source, an organic magnesium compound as a magnesium source, an organic gallium compound as a gallium source and high-purity oxygen as an oxygen source and using a metal organic compound chemical vapor deposition method.
And (3) transferring the substrate into a growth cavity of MOCVD equipment, regulating the initial temperature of the growth cavity to 500-800 ℃, controlling the vacuum degree of the growth cavity to 1x10 3Pa～4×103 Pa, introducing high-purity oxygen at a flow rate of 500-800 sccm, and controlling the growth time to 1-2 h.
According to the invention, through the modes of increasing the oxygen flow, increasing the oxygen partial pressure and reducing the oxygen defects, the prepared ZnMgGaO film has the characteristics of high crystallization quality, no phase separation, steep absorption cut-off edge and the like, and further the ZnMgGaO ultraviolet detector has lower dark current and faster light response speed.
The organic zinc compound takes high-purity nitrogen as carrier gas, and the flow rate of the carrier gas is 5-20 sccm; the organomagnesium compound takes high-purity nitrogen as carrier gas, and the flow rate of the carrier gas is 5-20 sccm; the organogallium compound uses high-purity nitrogen as carrier gas, and the carrier gas flow rate is 10-40 sccm.
The organic zinc compound is dimethyl zinc or diethyl zinc; the organic magnesium compound is dimethyl magnesium and/or diethyl magnesium; the organic gallium compound is trimethyl gallium and/or triethyl gallium.
Before step S1, the method may further include the following steps:
S0, cleaning the substrate.
The substrate was rinsed sequentially with trichloroethylene, acetone and ethanol and then dried with dry nitrogen.
S0 is an optional step, which may not be performed if the substrate is clean.
The step S1 further comprises the step of carrying out secondary annealing treatment on the ZnMgGaO film, and specifically comprises the following steps:
A. And (3) primary annealing: the ZnMgGaO film is moved into an annealing furnace, the nitrogen atmosphere is used, the nitrogen flow is 0.6-1.0 sccm, the furnace temperature of the annealing furnace is increased to 700-800 ℃ at the heating rate of 0.2-0.4 ℃/s, and after the temperature is kept constant for 3-5 min, the ZnMgGaO film is removed from the annealing furnace.
The annealing time of the first annealing is 3-5 min.
B. And (3) secondary annealing: and (3) reducing the temperature of the annealing furnace to 500-600 ℃, moving the ZnMgGaO film into the annealing furnace, and removing the ZnMgGaO film from the annealing furnace after keeping the temperature constant for 15-20 min.
The annealing time of the second annealing is 15-20 min.
The performance of the ZnMgGaO film can be increased by carrying out nitrogen annealing treatment on the ZnMgGaO film, so that the performance of the ZnMgGaO ultraviolet detector is increased, and the ZnMgGaO ultraviolet detector has lower dark current and faster light response speed.
S2, forming an interdigital electrode mask on the ZnMgGaO film by using negative photoresist lithography, and removing the interdigital electrode mask after sputtering metal on the interdigital electrode mask to form the interdigital electrode.
Forming an interdigital electrode mask on the ZnMgGaO film by using negative photoresist lithography, sputtering metal (such as gold and silver) on the interdigital electrode mask by using a small-sized film plating machine, and removing the interdigital electrode mask to form the interdigital electrode.
The sputtering current of the small-sized film plating machine is 5-8 mA.
The mode of removing the interdigital electrode mask can be ultrasonic mode, the ultrasonic time is 3-5 min, and the thickness of the formed interdigital electrode is 20-40 nm.
And S3, pressing In particles on the interdigital electrodes to obtain the ZnMgGaO ultraviolet detector with the MSM structure.
The preparation method and the performance of the ZnMgGaO ultraviolet detector provided by the invention are described in detail below by using a few specific examples.
Example 1
And placing the cleaned sapphire substrate into a growth cavity of MOCVD equipment, and regulating the growth temperature to 800 ℃ and the pressure to 4000Pa. Using dimethyl zinc as a zinc source, dimethyl magnesium dichloride as a magnesium source, trimethyl gallium as a gallium source, wherein the flow rate of carrier gas of the zinc source is 5sccm, the flow rate of carrier gas of the magnesium source is 5sccm, the flow rate of carrier gas of the gallium source is 10sccm, the flow rate of high-purity oxygen is 500sccm, which is far greater than the flow rates of the zinc source, the magnesium source and the gallium source, growing for 1h, closing the organic source and the oxygen, and reducing the temperature of the substrate to room temperature at 0.6 ℃/s to obtain the ZnMgGaO film.
The ZnMgGaO film was transferred into an annealing furnace, the furnace temperature of the annealing furnace was raised to 800℃at a heating rate of 0.4℃per second using a nitrogen atmosphere at a nitrogen flow rate of 1.0sccm, after the temperature was kept constant for 5 minutes, the ZnMgGaO film was removed from the annealing furnace, the furnace temperature of the annealing furnace was lowered to 600℃and then the ZnMgGaO film was transferred into the annealing furnace, after the temperature was kept constant for 20 minutes, the ZnMgGaO film was removed from the annealing furnace.
A negative photoresist lithography was used to form 50 pairs of interdigital electrode masks with a pitch of 10 μm and a length of 500 μm on ZnMgGaO films. And (3) putting the ZnMgGaO film photoetched with the interdigital electrode mask into a small film plating machine, sputtering metal gold under the condition that the pressure is 8Pa and the current is 6mA, removing the interdigital electrode mask through ultrasound to obtain an interdigital electrode, and pressing In particles on the interdigital electrode to obtain the ZnMgGaO ultraviolet detector with the MSM structure.
The film ZnMgGaO obtained in example 1 was subjected to uv-vis absorption spectrum test, and the spectrum is shown in fig. 3, and it can be seen from fig. 3 that the prepared ZnMgGaO film has a steep single light absorption cut-off edge, and the light absorption cut-off edge is about 235nm and is located in the solar blind uv band.
EDS test was performed on ZnMgGaO film obtained in example 1, and the graph is shown in FIG. 4. As can be seen from FIG. 4, zinc element, magnesium element and gallium element are simultaneously present in ZnMgGaO film prepared, and the ratio of the three elements is about 1:4:4.
The current-voltage characteristics and I-T characteristics of the ZnMgGaO ultraviolet detector obtained in example 1 under dark state and under 254nm light were tested, and the obtained spectra are shown in fig. 5 and 6, respectively. As can be seen from fig. 5 and fig. 6, the dark current of the prepared ZnMgGaO ultraviolet detector at 10V is about 24pA, the photocurrent is 0.5mA, the light-dark suppression ratio is 2.1×10 7, and the light response speed is faster, which indicates that the prepared ZnMgGaO ultraviolet detector has higher electrical property.
Example 2
Placing the cleaned sapphire substrate into a growth cavity of MOCVD equipment, and regulating the growth temperature to 800 ℃ and the pressure to 3000Pa. Using diethyl zinc as a zinc source, dimethyl magnesium dichloride as a magnesium source, triethyl gallium as a gallium source, wherein the flow rate of carrier gas of the zinc source is 10sccm, the flow rate of carrier gas of the magnesium source is 10sccm, the flow rate of carrier gas of the gallium source is 40sccm, the flow rate of high-purity oxygen is 800sccm which is far greater than the flow rates of the zinc source, the magnesium source and the gallium source, growing for 1.5h, closing the organic source and the oxygen, and reducing the temperature of the substrate to room temperature at 0.6 ℃/s to obtain the ZnMgGaO film.
The ZnMgGaO film was transferred into an annealing furnace, the furnace temperature of the annealing furnace was raised to 700℃at a heating rate of 0.2℃per second using a nitrogen atmosphere at a nitrogen flow rate of 0.6sccm, after the temperature was kept constant for 3 minutes, the ZnMgGaO film was removed from the annealing furnace, the furnace temperature was lowered to 500℃and then the ZnMgGaO film was transferred into the annealing furnace, and after the temperature was kept constant for 15 minutes, the ZnMgGaO film was removed from the annealing furnace.
A negative photoresist lithography was used to form 50 pairs of interdigital electrode masks with a pitch of 10 μm and a length of 500 μm on ZnMgGaO films. And (3) putting the ZnMgGaO film photoetched with the interdigital electrode mask into a small film plating machine, sputtering metal gold under the condition that the pressure is 8Pa, removing the interdigital electrode mask through ultrasound to obtain an interdigital electrode, and pressing In particles on the interdigital electrode to obtain the ZnMgGaO ultraviolet detector with the MSM structure.
The film ZnMgGaO obtained in example 2 was subjected to uv-vis absorption spectrum test, and the spectrum was shown in fig. 7, and it can be seen from fig. 7 that the prepared ZnMgGaO film has a steep single light absorption cut-off edge, and the light absorption cut-off edge is about 250nm and is located in the solar blind uv band.
EDS test was performed on ZnMgGaO film obtained in example 2, and the graph is shown in FIG. 8, and it can be seen from FIG. 8 that zinc element, magnesium element and gallium element are simultaneously present in ZnMgGaO film, and the ratio of the three elements is about 5:3:93.
The current-voltage characteristics and I-T characteristics of the ZnMgGaO ultraviolet detector obtained in example 2 under dark state and under 254nm light were tested, and the obtained spectra are shown in fig. 9 and 10, respectively. As can be seen from fig. 9 and 10, the dark current of the prepared ZnMgGaO ultraviolet detector under V is about 6pA, the photocurrent is 250nA, the light-dark suppression ratio is 4.2x10 5, and the light response speed is faster, which indicates that the prepared ZnMgGaO ultraviolet detector has higher electrical performance.
Example 3
Placing the cleaned sapphire substrate into a growth cavity of MOCVD equipment, and regulating the growth temperature to 600 ℃ and the pressure to 1000Pa. Dimethyl zinc is used as a zinc source, dimethyl magnesium and diethyl magnesium are used as magnesium sources, trimethyl gallium and triethyl gallium are used as gallium sources, the flow rate of carrier gas of the zinc sources is 5sccm, the flow rate of carrier gas of the magnesium sources is 5sccm, the flow rate of carrier gas of the gallium sources is 30sccm, the flow rate of high-purity oxygen is 500sccm and is far greater than the flow rates of the zinc sources, the magnesium sources and the gallium sources, the growth is carried out for 2 hours, the organic sources and the oxygen are closed, and the temperature of the substrate is reduced to room temperature at 0.6 ℃/s, so that ZnMgGaO films are obtained.
The ZnMgGaO film was transferred into an annealing furnace, the furnace temperature of the annealing furnace was raised to 750℃at a heating rate of 0.3℃per second using a nitrogen atmosphere at a nitrogen flow rate of 0.8sccm, after the temperature was kept constant for 4 minutes, the ZnMgGaO film was removed from the annealing furnace, the furnace temperature of the annealing furnace was lowered to 550℃and then the ZnMgGaO film was transferred into the annealing furnace, after the temperature was kept constant for 17 minutes, the ZnMgGaO film was removed from the annealing furnace.
A negative photoresist lithography was used to form 50 pairs of interdigital electrode masks with a pitch of 10 μm and a length of 500 μm on ZnMgGaO films. And (3) putting the ZnMgGaO film photoetched with the interdigital electrode mask into a small film plating machine, sputtering metal gold under the condition that the pressure is 6Pa, removing the interdigital electrode mask through ultrasound to obtain an interdigital electrode, and pressing In particles on the interdigital electrode to obtain the ZnMgGaO ultraviolet detector with the MSM structure.
The film ZnMgGaO obtained in example 3 was subjected to uv-vis absorption spectrum test, and the spectrum was shown in fig. 11, and it can be seen from fig. 11 that the prepared ZnMgGaO film has a steep single light absorption cut-off edge, and the light absorption cut-off edge is about 248nm and is located in the solar blind uv band.
EDS test was performed on ZnMgGaO film obtained in example 3, and the graph is shown in FIG. 12, and it can be seen from FIG. 12 that zinc element, magnesium element and gallium element are simultaneously present in ZnMgGaO film, and the ratio of the three elements is about 7:24:68. Current-voltage characteristics and I-T characteristics of the ZnMgGaO ultraviolet detector obtained in example 3 under dark state and under 254nm light were tested, and the obtained spectra are shown in FIG. 13 and FIG. 14, respectively. As can be seen from fig. 13 and 14, the dark current of the prepared ZnMgGaO uv detector at 10V is about 5.5pA, the photocurrent is 600nA, the light-dark suppression ratio is 1.1x10 5, and the photo-response speed is faster, which indicates that the prepared ZnMgGaO uv detector has higher electrical performance.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
The above embodiments of the present invention do not limit the scope of the present invention. Any of the various other corresponding changes and modifications made by the technical idea of the present invention should be included in the scope of the claims of the present invention.
Claims (3)
1. The preparation method of the ZnMgGaO ultraviolet detector is characterized in that the ZnMgGaO ultraviolet detector comprises a substrate, a ZnMgGaO film and interdigital electrodes which are sequentially overlapped from bottom to top;
The ZnMgGaO film is of a spinel structure;
The preparation method of the ZnMgGaO ultraviolet detector comprises the following steps:
S1, growing ZnMgGaO films on the surface of a substrate by using a metal organic compound chemical vapor deposition method by taking an organic zinc compound as a zinc source, an organic magnesium compound as a magnesium source, an organic gallium compound as a gallium source and high-purity oxygen as an oxygen source;
s2, forming an interdigital electrode mask on the ZnMgGaO film by using negative photoresist lithography, and removing the interdigital electrode mask after sputtering metal on the interdigital electrode mask to form an interdigital electrode;
S3, pressing In particles on the interdigital electrode to obtain a ZnMgGaO ultraviolet detector with an MSM structure;
placing a substrate into a growth cavity of MOCVD equipment, regulating the growth temperature to 800 ℃, controlling the pressure to 4000Pa, using dimethyl zinc as a zinc source, dimethyl magnesium dichloride as a magnesium source, trimethyl gallium as a gallium source, enabling the carrier gas flow rate of the zinc source to be 5sccm, enabling the carrier gas flow rate of the magnesium source to be 5sccm, enabling the carrier gas flow rate of the gallium source to be 10sccm, enabling the flow rate of high-purity oxygen to be 500sccm, growing for 1h, closing an organic source and oxygen, and reducing the temperature of the substrate to room temperature at 0.6 ℃/s to obtain ZnMgGaO films;
in the step S2, the sputtering current is 6mA, and the sputtering metal is gold;
The step S1 is further followed by a secondary annealing step, which is specifically as follows:
The ZnMgGaO film was transferred into an annealing furnace, the furnace temperature of the annealing furnace was raised to 800℃at a heating rate of 0.4℃per second using a nitrogen atmosphere at a nitrogen flow rate of 1.0sccm, after the temperature was kept constant for 5 minutes, the ZnMgGaO film was removed from the annealing furnace, the furnace temperature of the annealing furnace was lowered to 600℃and then the ZnMgGaO film was transferred into the annealing furnace, after the temperature was kept constant for 20 minutes, the ZnMgGaO film was removed from the annealing furnace.
2. The method of manufacturing a ZnMgGaO ultraviolet detector of claim 1, wherein the absorption cut-off edge of the ZnMgGaO film is 220-280 nm, and the light response cut-off edge of the ZnMgGaO ultraviolet detector is 220-270 nm.
3. The method of manufacturing a ZnMgGaO ultraviolet detector according to claim 1, wherein in the step S2, the interdigital electrode mask is removed by ultrasonic waves for 3 to 5 minutes.
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